Meso/macroporous γ-Al2O3 fabricated by thermal decomposition of nanorods ammonium aluminium carbonate hydroxide

Through exploring the reaction parameters during the synthesis of the AACH, rod-like ammonium aluminium carbonate hydroxide (AACH) with high crystallinity has been successfully prepared via a facile hydrothermal method. The synthesis parameters like time, the molar ratio of NH₄HCO₃/Al and the properties of starting materials were systematically investigated. The structure was characterized using X-ray powder diffraction (XRD), scanning electron microscopy (SEM), IR and transmission electron microscopy (TEM). The experimental results display that the obtained γ-Al₂O₃ materials possess meso/macroporosity and large pore volume, which are mainly attributed to the removal of gas molecules during the decomposition of AACH. Moreover, using the rod-like AACH as precursor, γ-Al₂O₃ nanorods were obtained via a low-temperature thermal decomposition method.     

Influence of Al2O3 support on the thermal decomposition of ammonium metavanadate

The thermal decomposition of ammonium metavanadate (AMV) supported on aluminium oxide was investigated using differential thermal analysis, thermogravimetry, infrared and X-ray diffraction techniques. The results obtained revealed that the decomposition of AMV supported on alumina proceeded in three decomposition stages. Alumina was found to enhance only the decomposition of the intermediate ammonium hexavanadate to produce V₂O₅. In addition, the values of activation energies of the various decomposition stages were accompanied by a significant decrease on decreasing the concentration of AMV. The infrared spectra indicated that the band corresponds to the surface site V=O strongly affected by the presence of Al₂O₃. Finally, an interaction between Al₂O₃ and V₂O₅ occurred at 660 °C giving well-crystallized AlVO₄.     

Characterizations of trimetallic heteronuclear Bi1−x La x [Fe(CN)6]·n(H2O) complexes and their thermal decomposition products

Heteronuclear Bi_1−x La _x [Fe(CN)₆]·nH₂O complexes were synthesized, and their crystal structures and thermal decomposition process were investigated by X-ray diffraction (XRD), thermogravimetry analysis (TGA), Auger electron spectroscopy (AES) with scanning electron microscope (SEM), and transmission electron microscopy (TEM). The crystal system of the complexes was orthorhombic having n = 4 for x = 0–0.7 and was hexagonal having n = 5 for x = 1.0. Their mixture was confirmed for x = 0.8 and 0.9. The lattice parameters for the orthorhombic increased with increasing the x value for the complexes. The single phase of trimetallic perovskite-type Bi_1−x La _x FeO₃ was obtained by its thermal decomposition at low temperature. The crystal system was hexagonal for BiFeO₃ (x = 0) and orthorhombic for x = 0.1–1.0. In the case of the decomposed perovskite sample, the lattice parameters decreased with increasing x values for Bi_1−x La _x FeO₃. The particle size was ca. 30 nm for Bi_0.2La_0.8FeO₃ obtained by thermal decomposition at 500 °C and it grew with an increase in decomposition temperature. For the Bi_0.5La_0.5FeO₃, AES showed that the elemental distributions of Bi, La, and Fe on the surface were very homogeneous for the sample decomposed at 700 °C.     

Preparation of YBa2Cu3O7−x by thermal decomposition of coprecipitated oxalates

Yttrium, barium and copper oxalates are coprecipitated quantitatively from metal acetate solutions with oxalic acid in water-acetone mixtures. The particle-size distribution of the precipitate can be controlled by the precipitation conditions. Thermal decomposition of the coprecipitate leads to single-phase YBa₂Cu₃O_7-x . Despite the intermediate formation of BaCO₃, the minimal reaction temperature (770 °C) is clearly lower than that for the solid-state reaction. Results of differential thermal analysis and isothermal thermogravimetry are discussed. The products are characterized by X-ray diffraction and infrared spectroscopy.     

Preparation and thermal decomposition of hexa-ammonium tetraphosphate dihydrate(NH4)6P4O13·2H2O

Hexa-ammonium tetraphosphate dihydrate, (NH4)6P4O13·2H2O (HATP), was prepared by the hydrolysis of sodium cyclo-tetraphosphate with sodium hydroxide solution, followed by ion-exchange with ammonium. Thermal decomposition in static air was first carried out dynamically, at a heating rate of 5 K min-1 as used in thermal analysis (thermogravimetric-differential thermal analysis), and also isothermally. To examine the effect of humidity on the thermal decomposition, HATP was heated isothermally in streams of dry and humid air. The products were characterized by X-ray diffraction analysis and high-performance liquid chromatography–flow injection analysis. At 100°C, HATP was decomposed to mono- and triphosphates and to 2 mol diphosphate, and this was accelerated by humidity. Further degradation of the triphosphate to mono- and diphosphates took place slowly. The 2 mol diphosphate also decomposed slowly to 4 mol monophosphate. At temperatures above 150°C, the form I of ammonium polyphosphate (I-APP) was produced. I-APP was further hydrolysed by humidity to shorter-chain phosphates, such as mono-, di- and triphosphates. This revised version was published online in November 2006 with corrections to the Cover Date.     

Crystal Structure of Double Co(NH3)6 3 + Np(V) Malonates Co(NH3)6(NpO2C3H2O4)2A·H2O (A = OH and NO3)

X-ray diffraction analysis of Co(NH₃)₆(NpO₂C₃H₂O₄)₂NO₃·H₂O (I) and Co(NH₃)₆(NpO₂· C₃H₂O₄)₂OH·H₂O (II) showed that they consist of [NpO₂C₃H₂O₄] _n ^{n -} infinite anionic chains, [Co(NH₃)₆]^{3 +} cations, NO₃ ^- (I) and OH^- (II) anions, and molecules of crystallization water. The anionic chain structure is similar to that in the known compound Co(NH₃)₆(NpO₂C₃H₂O₄)₂C₃H₃O₄. Neptunium(V) atoms occur in hexagonal-bipyramidal environment. The coordination capacity of malonate anions is 6, and they simultaneously coordinate three neptunyl(V) cations NpO₂ ⁺ in the chain.     

Synthesis of hexagonal Al2−x Cr x O3 nanodisks by a thermal decomposition of mesoporous Cr4+:Al2O3 powders

Monodispersed hexagonal Al_2−x Cr _x O₃ nanodisks are synthesized through a reactive doping of Cr⁶⁺ cations in a hydrogenated mesoporous AlO(OH)·αH₂O powder followed by annealing at 1,200 °C in air. The reaction was carried out by a drop wise addition of an aqueous Cr⁶⁺ solution (0.5–1.0 M) to AlO(OH)·αH₂O, at room temperature. Al_2−x Cr _x O₃ nanostructure formation was controlled by the nucleation and growth from the intermediate amorphous mesoporous Cr⁴⁺:Al₂O₃ composites in the temperature range 400–1,000 °C. The nanodisks of ∼50 nm diameter and thickness of ∼16 nm is observed in the sample with x of 0.2 and similar nanodisks with a low dimension is observed at a higher value of x of 1.6 (after 2 h of heating at 1,200 °C). The Cr³⁺ ↔ Al³⁺ substitution, x ≤ 1.2, inhibits grain growth in small crystallites. The crystallites in x = 0.2 composition have 43 nm diameter while it is 15 nm in those with x = 1.2 composition.     

Effect of sintering on the magnetization behaviour of Mg x Zn(1 −x)Fe2O4 system

Magnesium zinc ferrites with the general formula Mg _x Zn_{(1 −x)}Fe₂O₄ were prepared by the standard ceramic technology route involving double sintering. X-ray analysis was carried out to confirm the single-phase formation as well as to calculate the lattice parameters. Two sets of samples were prepared by sintering the samples at 1100°C for 15 and 30 h respectively. The high-field loop tracer was used to measure the hysteresis parameters. It is observed that the sintering conditions effectively modify the magnetization characteristics of these ferrites.     

Lattice variation and thermal parameters of Ni x Mg1−x SO4·7H2O single crystals

Ni _x Mg_1−x SO₄·7H₂O single crystals were grown by the slow evaporation method from aqueous solutions. Density was measured by the floatation method. X-ray diffraction data were collected for powder samples and used for the estimation of lattice variation and thermal parameters like Debye-Waller factor, mean-square amplitude of vibration and Debye temperature. Lattice volumes approximately obey a relation similar to Retger’s rule. Values of thermal parameters do not follow any particular order with composition. The results obtained are reported.     

退火处理对硼酸镁晶须增强铝基复合材料性能的影响

采用挤压铸造方法制备了硼酸镁晶须增强纯铝基复合材料,在450℃下对其进行了不同时间的退火处理,研究了不同退火时间对复合材料的室温力学性能、热膨胀行为及基体织构的影响.试验结果表明,退火处理能有效提高复合材料的抗拉强度,随着退火时间的增加材料的拉伸强度也逐渐增加,在5 h时达到最大值295 MPa,7 h时略有下降,为285 MPa.复合材料的热膨胀曲线表明,退火处理会使材料的热膨胀系数变大,随着退火时间的增加,材料的热膨胀系数先增加后减小,但始终高于未退火处理的材料.     

Preparation,structural and spectroscopic studies of (YxLu1−x)2O3:Eu3+ nanopowders

Lutetium and yttrium oxides are promising scintillating materials suitable for use in medical planar X-ray imaging and mammography. In this paper the procedure for preparation of europium doped mixed lutetium–yttrium oxide nanopowders using polymer complex solution synthesis method is presented. Detailed information on nanopowder phase, morphology and crystallinity are obtained using X-ray powder diffraction, SEM and TEM while optical properties are investigated by photoluminescence and radioluminescence measurements. Constituting nanoparticles are 20–40 nm in size, and have excellent structural ordering in cubic bixbyite-type. Unit cell parameter, ionic coordinates, crystal coherence size and microstrain are determined from Rietveld analysis. All powders show strong Eu³⁺-characteristic red emission, with an average ⁵D₀ emission lifetime of 1.5 ms. Radioluminescence efficiency is about 15% of the commercial micron-sized Gd₂O₂S:Eu³⁺ powder while negligible level of afterglow is found.     

不同镁源反应物对反应烧结制备Pb（Mg1/3Nb2/3）O3陶瓷的影响

采用MgO和(MgCO3)4·Mg(OH)2·5H2O为不同镁源反应物,通过高温反应烧结工艺制备Pb(Mg1/3Nb2/3)O0.(PMN)陶瓷,研究不同Mg源反应物对PMN陶瓷物相组成、相对密度及组织形貌的影响.结果表明:以MgO为前驱体时.由于其反应活性差,扩散和反应不均匀,导致烧结样品中有焦绿石相残留,且焦绿石相对晶界的钉扎阻碍作用使得致密化过程进行相对较慢,所得PMN样品致密度相对较低;而以(MgCO3)4·Mg(OH)2·5H2O为前驱体时,因其受热分解可以得到大比表面积、高反应活性的MgO,从而可以制得高致密度且具有单一钙钛矿相组成的PMN陶瓷材料.     

Synthesis and structural study of new potassium uranyl selenates K2(H5O2)(H3O)[(UO2)2(SeO4)4(H2O)2](H2O)4 and K3(H3O)[(UO2)2(SeO4)4(H2O)2](H2O)5

Single crystals of new uranyl selenates K₂(H₅O₂)(H₃O)[(UO₂)₂(SeO₄)₄(H₂O)₂](H₂O)₄ (1) and K₃(H₃O)[(UO₂)₂(SeO₄)₄(H₂O)₂](H₂O)₅ (2) were prepared by isothermal evaporation at room temperature. The crystal structure of 1 was solved by the direct method [C2/c, a = 17.879(5), b = 8.152(5), c = 17.872(5) Å, β = 96.943(5)°, V = 2585.7(19) ų, Z = 4] and refined to R ₁ = 0.0449 (wR ₂ = 0.0952) for 2600 reflections with |F _o| ≥ 4σ _F . The structure of 2 was solved by the direct method [P2₁/c, a = 17.8377(5), b = 8.1478(5), c = 23.696(1) Å, β = 131.622(2)°, V = 2574.5(2) ų, Z = 4] and refined to R ₁ = 0.0516 (wR ₂ = 0.1233) for 4075 reflections with |F _o| ≥ 4σ _F . The structures of 1 and 2 are based on [(UO₂)₂(SeO₄)₄(H₂O)₂]^4? layers. The charge of the inorganic layer is compensated by potassium and oxonium ions arranged in the interlayer space. Each K ion is surrounded by seven O atoms belonging to uranyl selenate layers and water molecules, so that it binds with each other the adjacent uranyl selenate structural elements.